US7214256B2 - Solvent extraction process - Google Patents

Solvent extraction process Download PDF

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Publication number
US7214256B2
US7214256B2 US10/631,299 US63129903A US7214256B2 US 7214256 B2 US7214256 B2 US 7214256B2 US 63129903 A US63129903 A US 63129903A US 7214256 B2 US7214256 B2 US 7214256B2
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extraction
metal
stage
solution
organic
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US20040103756A1 (en
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Gary A. Kordosky
Hans Hein Steger
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Cognis IP Management GmbH
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Cognis Corp
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Application filed by Cognis Corp filed Critical Cognis Corp
Priority to US10/631,299 priority Critical patent/US7214256B2/en
Priority to PCT/US2003/024430 priority patent/WO2004022604A2/en
Priority to ES200550014A priority patent/ES2283206A1/es
Priority to BRPI0313904-2B1A priority patent/BR0313904B1/pt
Priority to CN038208709A priority patent/CN1678763B/zh
Priority to AU2003258054A priority patent/AU2003258054B2/en
Priority to RU2005109425/02A priority patent/RU2005109425A/ru
Priority to MXPA05002094A priority patent/MXPA05002094A/es
Priority to PE2003001251A priority patent/PE20050063A1/es
Assigned to COGNIS CORPORATION (COGNIS CORP.) reassignment COGNIS CORPORATION (COGNIS CORP.) ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HEIN STEGER, HANS, KORDOSKY, GARY A.
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/30—Oximes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/02—Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • This invention relates to a solvent extraction process for the recovery of metals from aqueous solutions.
  • Solvent extraction is a widely used technology for the recovery of metals from aqueous solutions containing the metals.
  • One of the more common staging configurations in metal recovery is two extraction stages in combination with two strip stages for a total of four stages.
  • This new staging arrangement gives both higher metal recovery and more effective use of the organic phase and the metal extraction reagents present therein when the staging arrangements are compared under the exact same conditions.
  • the present invention does not increase capital costs since the total number of stages and the size of the plants are exactly the same in both staging arrangements.
  • FIG. 1 shows a known staging arrangement in which two extraction stages are present in combination with two stripping stages.
  • FIG. 2 shows the staging arrangement of the invention in which three extraction stages are present in combination with one strip stage.
  • the present invention is not dependent on the particular metals present in the electrolyte solutions from which the metals are to be extracted.
  • different leach solutions can be used with respect to the metal ores.
  • nickel ores are typically leached with ammonia, extracted from the ammonia solutions, and stripped with acid to form an aqueous acidic electrolyte solution used in an electrowinning step.
  • the solvent extraction process (SX process) for extracting metals such as copper typically involves the following steps, (plus a wash stage), which result in electrolyte solutions used in electrowinning copper metal.
  • Other processes that include solvent extraction and stripping can be employed in accordance with the invention with other metals such as nickel, zinc and the like to produce an electrolyte from which their respective metals are electrowon:
  • Leach Solution from step 1 above enters Extraction Stage 1 where it is mixed with Organic (the water-immiscible organic solvent containing the oxime extraction reagent) from Extraction Stage 2.
  • Organic the water-immiscible organic solvent containing the oxime extraction reagent
  • Loaded Organic which is the organic solvent containing the copper-extractant complex in solution
  • Strip Stage 1 is sent to Strip Stage 1, where it is contacted with Electrolyte (aqueous acid strip solution) from Strip Stage 2.
  • Electrolyte aqueous acid strip solution
  • Leach Solution enters Extraction Stage 1, where it is mixed with Organic from Extraction Stage 2.
  • Loaded Organic exits Extraction Stage 1 and enters the Strip Stage where it is contacted with Barren Electrolyte.
  • Pregnant Electrolyte exits the Strip Stage for further processing by electrowinning.
  • Stripped Organic leaves the Strip Stage and enters Extraction Stage 3, where it is contacted with Aqueous (partially extracted leach solution) from Extraction Stage 2.
  • Aqueous Raffinate is removed from Extraction Stage 3.
  • Organic from Extraction Stage 3 is sent to Extraction Stage 2, where it is contacted with Aqueous from Extraction Stage 1.
  • circuit configuration shown in FIG. 2 can be used in one or more trains, depending on the size of the plant. Also, the circuit configuration shown in FIG. 2 can be used with one or more wash stages, preferably a single wash stage.
  • This example compares a copper solvent extraction circuit having 2 extraction stages and 2 stripping stages (2E, 2S) with a copper solvent extraction circuit having 3 extraction stages and 1 strip stage (3E, 1S).
  • An extraction isotherm was generated using an organic solution 0.296 molar in 5-nonyl-2-hydroxyacetophenone oxime (ketoxime) and 0.0964 molar in 5-nonylsalicylaldoxime (aldoxime) in a hydrocarbon diluent.
  • the aqueous copper leach solution contained 6.36 g/l Cu and 150 g/l sulfate ion as sodium sulfate at a pH of 1.67.
  • the above organic solution was first contacted several times with an aqueous solution having about 39 g/l Cu and 168 g/l sulfuric acid to obtain a preliminary stripped organic phase containing 1.37 g/l Cu.
  • This preliminary stripped organic phase was then contacted vigorously with the copper leach solution at various organic to aqueous (O/A) ratios for sufficient time to obtain equilibrium.
  • the resulting equilibrated organic phases were analyzed by atomic absorption for copper and iron while the resulting equilibrium aqueous phases were analyzed by atomic absorption for copper only. The results are given in Table 1 below.
  • the stripped organic values that were used in the Cognis Isocalc computer program were obtained by equilibrating the organic with an aqueous solution to give a copper stripped organic value circuit is representative for either one or two stripping stages depending on the particular circuit simulation.
  • two sets of stripping conditions were used.
  • the barren stripping solution had 35 g/l Cu and 180 g/l sulfuric acid building to a pregnant strip solution of about 50 g/l Cu and 157 g/l sulfuric acid.
  • the barren stripping solution had 35 g/l Cu and 150 g/l sulfuric acid building to a pregnant strip solution of about 50 g/l Cu and 127 g/l sulfuric acid.
  • Simulated circuits were run with the computer program at various advance organic/aqueous (O/A) ratios to compare the results obtained with 3 extraction and 1 stripping stage verses the results obtained with 2 extraction and 2 stripping stages.
  • a circuit having 3 extraction and 1 strip stage will result in higher copper recovery than a circuit having 2 extraction and 2 strip stages when the circuits are compared under exactly the same conditions. For example compare 1d (96.6% Cu recovery) with 1a (95.0% Cu recovery) and 1e (90.7% Cu recovery) with 1c (86.8% Cu recovery). Also compare 2d (95.2% Cu recovery) with 2a (94.1% Cu recovery) and 2e (90.7% Cu recovery) with 2c (88.2% Cu recovery).
  • the Net Transfer (g/l Cu/vol %) of the reagent is higher in the 3E, 1S staging than in the comparable 2E, 2S staging, showing that the reagent is used more efficiently in the 3E, 1S staging than in the 2E, 2S staging.
  • a second aspect of the 3E, 1 S stage configuration that is a favorable over the 2E, 2S stage configuration is enhanced copper over iron (Cu/Fe) selectivity.
  • Cu/Fe copper over iron
  • the Cu/Fe selectivity is calculated as follows.
  • the copper transfer of the organic phase is divided by the iron loading of the loaded organic phase [(Loaded Organic Cu—Stripped Organic Cu)/Loaded Organic Fe].
  • the data in Table 3 shows that for any set of comparable conditions the 3E, 1S stage configuration shows better copper/iron (Cu/Fe) selectivity than the 2E, 2S stage configuration. For example compare set 1a with set 1d, set 1c with set 1e, set 2a with set 2d and set 2c with set 2e.
  • the higher Cu/Fe selectivity of the 3E, 1S stage configuration over the 2E, 2S stage configuration provides an added advantage for the 3E, 1S staging configuration over the 2E, 2S configuration.
  • Example 2 also compares a copper solvent extraction circuit having 2 extraction stages and 2 stripping stages (2E, 2S) with a copper solvent extraction circuit having 3 extraction stages and 1 strip stage (3E, 1 S).
  • the copper content of the leach solution was 61.37 g/l Cu at a pH of 1.8.
  • This leach solution is representative of a concentrate leach solution.
  • Two extraction isotherms were generated, one with 32 volume % LIX 84-I in a hydrocarbon diluent and one with 32 volume % LIX 984N reagent in a hydrocarbon diluent.
  • LIX 84-I is a copper solvent extraction reagent available from Cognis Corporation of Gulph Mills, Pa., whose active copper extractant is 5-nonyl-2-hydroxyacetophenone oxime at a concentration of 1.54 molar.
  • LIX 984N is a copper solvent extraction reagent available from Cognis Corporation whose active extractants are 5-nonyl-2-hydroxyacetophenone oxime (0.77 molar) and 5-nonylsalicylaldoxime (0.88 molar).
  • the respective organic solutions were contacted vigorously with the copper leach solution at various organic to aqueous (O/A) ratios for sufficient time to obtain equilibrium.
  • the resulting equilibrated organic phase and aqueous phases were analyzed by atomic absorption for copper. The results are set forth in Table 4 below.
  • mixer efficiencies are consistent with mixer efficiencies that are obtained in the 2E, 2S circuit and which can be obtained in a 3E, 1S circuit of the invention in modern copper solvent extraction plants operating at temperatures of about 35° C. which is the temperature at which concentrate leach solutions will enter the copper solvent extraction plant.
  • the stripped organic values that were used in the computer modeled circuit for LIX 84-I are consistent with stripped organic values that are obtained in operating copper solvent extraction plants when the barren strip solution has 30 g/l Cu and 168 g/l sulfuric acid and the pregnant strip solution has about 45 g/l Cu and 146 g/l sulfuric acid.
  • the stripped organic values that were used for LIX 984N are consistent with the stripped organic values that are obtained in a plant when the barren strip solution has 35 g/l Cu and 180 g/l acid and the pregnant strip solution has 45 g/l Cu and 165 g/l sulfuric acid.
  • the cost to install a mixer/settler tank is about US $400 per square foot of settler area on a fully prepared site.
  • a single mixer settler unit of this size would cost about US $3.24 million without considering site preparation costs. If each mixer settler unit needed to be 25% larger the cost would be 4.05 million dollars per mixer settler unit giving a total increase in capital for the 2E, 2S stage configuration of US $3.24 million over the 3E, 1S stage configuration.
  • this Example 3 compares a copper solvent extraction circuit having 2 extraction stages and 2 stripping stages (2E, 2S) with a copper solvent extraction circuit having 3 extraction and 1 strip stage (3E, 1S).
  • the copper content of the leach solution is 4.57 g/l Cu at a pH of 1.8.
  • This leach solution is representative of heap leach solutions commonly found in copper heap leaching operations.
  • An extraction isotherm was generated with a solution of 0.225 molar 5-nonyl-2-hydroxyacetophenone oxime in a hydrocarbon diluent.
  • the respective organic solution was contacted vigorously with the copper leach solution at various organic to aqueous (O/A) ratios for sufficient time to obtain equilibrium.
  • the stripped organic values that were used in the computer modeling program are consistent with stripped organic values that are obtained in operating copper solvent extractions plants when the barren strip solution has 35 g/l Cu and 180 g/l acid and the pregnant strip solution has 50 g/l Cu and 157 g/l sulfuric acid.
  • this example compares a copper solvent extraction circuit having 2 extraction stages and 2 stripping stages (2E, 2S) with a copper solvent extraction circuit having 3 extraction and 1 strip stage (3E, 1 S).
  • the leach solution has 5.97 g/l Cu, 2.7 g/l Fe at a pH of 2.0.
  • the organic solution contained about 0.194 molar 5-nonyl-2-hydroxyacetophenone oxime, about 0.189 molar 5-nonylsalicylaldoxime and about 28.2 g/l of the equilibrium modifier dodecanone all in the hydrocarbon diluent SHELLSOLTM D70.
  • the respective organic solution was contacted vigorously with the copper leach solution at various organic to aqueous (O/A) ratios for sufficient time to obtain equilibrium.
  • the resulting equilibrated organic phases were analyzed for copper and iron while the aqueous phases were analyzed for copper. Analysis was by atomic absorption. The results are given in Table 8 below.
  • the stripped organic values that were used in the computer modeled circuit are consistent with stripped organic values that are obtained in operating copper solvent extraction plants when the barren strip solution has 35 g/l Cu and 180 g/l acid and the pregnant strip solution has 50 g/l Cu and 157 g/l sulfuric acid.
  • the results of the computer simulations are shown in Table 9.
  • Example 1 compare the Cu/Fe selectivity for the 2E, 2S sets in Table 9 with the Cu/Fe selectivity for similar 3E, 1S sets in Table 9.
  • the iron loading in the organic phase for each isotherm point is plotted against the copper loading for the same point.
  • the resulting graph was then used to obtain an iron loading for any copper loading of the organic phase.
  • the loaded organic was obtained from the computer simulated circuit run and then the iron loading for that copper loaded organic was obtained from the graph of iron loading verses copper loading.
  • This Cu/Fe selectivity data for the sets in Table 9 is given in Table 10 below.
  • Cu/Fe selectivity was calculated by dividing the copper transfer of the organic phase by the iron loading on the loaded organic phase [(Loaded Organic Cu—Stripped Organic Cu)/Loaded Organic Fe].
  • the data in Table 10 shows that for comparable conditions the 3E, 1S stage configuration results in higher Cu/Fe selectivity than the 2E, 2S stage configuration. For example, compare set 1a with set 1b, and set 2a with set 2b.
  • the higher Cu/Fe selectivity of the 3E, 1S stage configuration over the 2E, 2S stage configuration provides an added advantage of the 3E, 1S staging configuration over the 2E, 2S configuration.

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  • Metallurgy (AREA)
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US10/631,299 2002-09-03 2003-07-31 Solvent extraction process Expired - Lifetime US7214256B2 (en)

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Application Number Priority Date Filing Date Title
US10/631,299 US7214256B2 (en) 2002-09-03 2003-07-31 Solvent extraction process
RU2005109425/02A RU2005109425A (ru) 2002-09-03 2003-08-06 Способ экстракции растворителем
ES200550014A ES2283206A1 (es) 2002-09-03 2003-08-06 Proceso de extraccion con disolvente.
BRPI0313904-2B1A BR0313904B1 (pt) 2002-09-03 2003-08-06 Configuração de circuito para uma planta de extração de solvente de metal, método para aumentar a recuperação de metal em uma planta de extração de solvente de metal, planta de extração de solvente de metal para extrair metal de um minério metálico, e, processo de extração de solvente para extrair os metais de uma solução de lixívia aquosa que contém valores metálicos
CN038208709A CN1678763B (zh) 2002-09-03 2003-08-06 溶剂萃取方法
AU2003258054A AU2003258054B2 (en) 2002-09-03 2003-08-06 Solvent extraction process
PCT/US2003/024430 WO2004022604A2 (en) 2002-09-03 2003-08-06 Solvent extraction process
MXPA05002094A MXPA05002094A (es) 2002-09-03 2003-08-06 Proceso de extraccion de solvente.
PE2003001251A PE20050063A1 (es) 2003-07-31 2003-12-10 Proceso de extraccion por solvente de metales desde una solucion de lixiviacion acuosa

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060088458A1 (en) * 2004-10-04 2006-04-27 Kordosky Gary A Method for metal heap and dump leaching coupled with metal solvent extraction
US20090074639A1 (en) * 2007-09-17 2009-03-19 Phelps Dodge Corporation Controlled copper leach recovery circuit
US8420048B1 (en) 2011-12-20 2013-04-16 Freeport-Mcmoran Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US20140193317A1 (en) * 2013-01-10 2014-07-10 Bloom Energy Corporation Methods of Recovering Scandium from Titanium Residue Streams
US9169533B2 (en) 2011-12-20 2015-10-27 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
WO2020077026A1 (en) * 2018-10-12 2020-04-16 Basf Se Reagent compositions for metal solvent extraction and methods of preparation and use thereof

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CN102212687A (zh) * 2011-05-24 2011-10-12 钱峰 2-羟基-5-壬基苯乙酮肟在新型高效萃取剂中的应用
RU2481409C1 (ru) * 2011-12-08 2013-05-10 Лидия Алексеевна Воропанова Экстракция меди из водных растворов растительными маслами
CN105506636A (zh) * 2016-02-02 2016-04-20 深圳中能润德环保有限公司 一种萃取含铜废液的循环再生系统及方法
CN106191436B (zh) * 2016-09-18 2019-02-12 重庆康普化学工业股份有限公司 提高铜回收率的铜萃取工艺

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Cited By (22)

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Publication number Priority date Publication date Assignee Title
US7635457B2 (en) * 2004-10-04 2009-12-22 Cognis Ip Management Gmbh Method for heap and dump leaching coupled with solvent extraction for metal recovery
US20060088458A1 (en) * 2004-10-04 2006-04-27 Kordosky Gary A Method for metal heap and dump leaching coupled with metal solvent extraction
US8828353B2 (en) 2007-09-17 2014-09-09 Freeport Minerals Corporation Controlled copper leach recovery circuit
US20090074639A1 (en) * 2007-09-17 2009-03-19 Phelps Dodge Corporation Controlled copper leach recovery circuit
US8003064B2 (en) 2007-09-17 2011-08-23 Freeport-Mcmoran Corporation Controlled copper leach recovery circuit
US8372361B2 (en) 2007-09-17 2013-02-12 Freeport-Mcmoran Corporation Copper recovery circuit
US8372360B2 (en) 2007-09-17 2013-02-12 Freeport-Mcmoran Corporation Controlled metal leach recovery circuit
US10036080B2 (en) 2011-12-20 2018-07-31 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US10036096B2 (en) 2011-12-20 2018-07-31 Freeport Minerals Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US9023313B2 (en) 2011-12-20 2015-05-05 Freeport Minerals Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US11932919B2 (en) 2011-12-20 2024-03-19 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US9169533B2 (en) 2011-12-20 2015-10-27 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US9447483B2 (en) 2011-12-20 2016-09-20 Freeport Minerals Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US9856570B2 (en) 2011-12-20 2018-01-02 Freeport Minerals Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US11584974B2 (en) 2011-12-20 2023-02-21 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US8420048B1 (en) 2011-12-20 2013-04-16 Freeport-Mcmoran Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US10501821B2 (en) 2011-12-20 2019-12-10 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US11053566B2 (en) 2011-12-20 2021-07-06 Freeport Minerals Corporation System and method including multi-circuit solution extraction for recovery of metal values from metal-bearing materials
US10793958B2 (en) 2011-12-20 2020-10-06 Freeport Minerals Corporation System and method for parallel solution extraction of one or more metal values from metal-bearing materials
US20140193317A1 (en) * 2013-01-10 2014-07-10 Bloom Energy Corporation Methods of Recovering Scandium from Titanium Residue Streams
US9102999B2 (en) * 2013-01-10 2015-08-11 Bloom Energy Corporation Methods of recovering scandium from titanium residue streams
WO2020077026A1 (en) * 2018-10-12 2020-04-16 Basf Se Reagent compositions for metal solvent extraction and methods of preparation and use thereof

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US20040103756A1 (en) 2004-06-03
BR0313904B1 (pt) 2013-12-17
RU2005109425A (ru) 2005-09-10
AU2003258054B2 (en) 2008-11-13
BR0313904A (pt) 2005-07-19
WO2004022604A3 (en) 2004-12-09
MXPA05002094A (es) 2005-06-06
AU2003258054A1 (en) 2004-03-29
ES2283206A1 (es) 2007-10-16
CN1678763B (zh) 2011-08-10
WO2004022604A2 (en) 2004-03-18

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